CN111537500B

CN111537500B - Method for identifying methanol solution of aldehyde oil

Info

Publication number: CN111537500B
Application number: CN202010159718.0A
Authority: CN
Inventors: 黄升; 黄志云; 刘明威; 邱伟杰; 袁莉莉
Original assignee: Nanhai Beisha Pharmaceutical Co ltd
Current assignee: Nanhai Beisha Pharmaceutical Co ltd
Priority date: 2020-07-06
Filing date: 2020-07-06
Publication date: 2022-11-25
Anticipated expiration: 2040-07-06
Also published as: CN111537500A

Abstract

The invention discloses a method for identifying an aldehyde oil methanol solution, which comprises the steps of carrying out aldehyde group identification and olefinic bond identification on a test sample, and judging the test sample to be the aldehyde oil methanol solution meeting the requirements if the test sample simultaneously passes the aldehyde group identification and the olefinic bond identification; and if the test sample cannot pass the aldehyde group identification and the olefinic bond identification at the same time, judging that the test sample does not meet the requirements.

Description

Method for identifying methanol solution of aldehyde oil

Technical Field

The invention relates to the technical field of medicament identification, in particular to a method for identifying an aldehyde oil methanol solution.

Background

The aldehyde oil methanol solution is dark red transparent liquid and is inflammable, vinyl ether, dimethylformamide and phosphorus trichloride are used as raw materials, kerosene is used as a solvent to carry out addition reaction to prepare aldehyde oil, anhydrous methanol is used for dilution, and petroleum ether is used for extraction and purification to obtain a medical intermediate.

The aldehyde oil methanol solution is a key intermediate raw material in the production process of sulfadiazine bulk drugs. The aldehyde oil methanol solution is a methanol solution of a mixture of dimethylamino propylene aldehyde methyl ether, the main component of the methanol solution is the dimethylamino propylene aldehyde methyl ether, and the dimethylamino propylene aldehyde methyl ether has no identification method of the product in international standards, national standards and industrial standards at present.

Disclosure of Invention

The invention aims to overcome the defects of the prior art and provide a simple, quick and high-accuracy method for identifying the methanol solution of the aldehyde oil.

In order to realize the above effects, the technical scheme adopted by the invention is as follows: a method for identifying aldehyde oil methanol solution is characterized in that aldehyde group identification and olefinic bond identification are carried out on a test sample, and if the test sample passes the aldehyde group identification and the olefinic bond identification at the same time, the test sample is judged to be the aldehyde oil methanol solution meeting the requirements; and if the test sample cannot pass the aldehyde group identification and the olefinic bond identification at the same time, judging that the test sample does not meet the requirement.

The aldehyde group identification comprises the following steps: taking a test sample solution, adding a 2, 4-dinitrophenylhydrazine test solution into the test sample solution, fully oscillating the test sample solution and the test sample solution, standing the test sample solution and the test sample solution, judging that the test sample passes aldehyde group identification if orange yellow precipitates are generated in the test sample solution, and judging that the test sample does not pass aldehyde group identification if no orange yellow precipitates are generated in the test sample solution.

The olefinic bond identification comprises the following steps: adding bromine carbon tetrachloride solution into a test tube, adding test sample solution, fully oscillating, judging that the test sample passes olefinic bond identification if the reddish brown color in the test tube fades, and judging that the test sample does not pass olefinic bond identification if the reddish brown color in the test tube does not fade.

Preferably, in the aldehyde group identification process, the volume ratio of the test sample to the 2, 4-dinitrophenylhydrazine test solution is 1.

Preferably, during said identification of the olefinic bond, the volume ratio of water, bromine in carbon tetrachloride and the test sample is 1.

Preferably, the formulation of the test sample: equal volume of aldehyde oil and methanol are taken and mixed evenly.

Preferably, the preparation of the 2, 4-dinitrophenylhydrazine test solution comprises the following steps: weighing 1.5g of 2, 4-dinitrophenylhydrazine, adding 20ml of sulfuric acid solution (1 → 2), dissolving, adding water to 100ml, and filtering to obtain a 2, 4-dinitrophenylhydrazine test solution.

Preferably, the preparation of the bromine in carbon tetrachloride solution: taking 1ml of bromine, placing the bromine into a glass bottle which is plugged by vaseline, adding 50ml of carbon tetrachloride, and forcibly shaking up to obtain a bromine carbon tetrachloride solution.

The invention has the beneficial effects that: the invention establishes a discrimination and inspection method according to the structural functional group analysis of dimethylamino propylene acetal methyl ethyl ether. The method can detect whether the sample contains aldehyde group and olefinic bond respectively by testing aldehyde group identification and olefinic bond identification of the test sample, and can avoid interference of impurities in the raw materials on the result because vinyl ether, dimethyl formamide and phosphorus trichloride which are used for preparing aldehyde oil do not simultaneously have aldehyde group and olefinic bond, so that the sample can be quickly identified by the identification method.

Drawings

FIG. 1 is a flow chart of the present invention.

FIG. 2 is a flow chart of aldehyde group identification in the present invention.

FIG. 3 is a flow chart of the olefinic bond identification in the present invention.

Detailed Description

The claimed embodiments of the present invention will now be described in further detail with reference to the accompanying drawings and specific examples.

Referring to fig. 1, the method for identifying an aldehyde oil methanol solution in the present embodiment includes performing aldehyde group identification and olefin group identification on a test sample, and in the present embodiment, the test sample is prepared as follows: 10ml of aldehyde oil solution is taken, 10ml of methanol is added, and the mixture is shaken up to obtain a test sample.

Referring to fig. 2, the aldehyde group identification in this example comprises the following steps: taking 1mL of test sample solution, adding 3mL of 2, 4-dinitrophenylhydrazine test solution into the test sample solution, fully oscillating the test sample solution and the test sample solution, standing the test sample solution and the test sample solution after fully oscillating the test sample solution and the test sample solution, judging that the test sample passes aldehyde group identification if orange yellow precipitate is generated in the test sample solution, and judging that the test sample does not pass aldehyde group identification if no orange yellow precipitate is generated in the test sample solution.

In this embodiment, the preparation process of the 2, 4-dinitrophenylhydrazine test solution is as follows: weighing 1.5g of 2, 4-dinitrophenylhydrazine, adding 20ml of sulfuric acid solution (prepared by adding water to 2 volumes of 1 volume of concentrated sulfuric acid), dissolving, adding water to 100ml, and filtering to obtain the 2, 4-dinitrophenylhydrazine test solution.

Referring to fig. 3, the olefinic bond identification includes the steps of: and (2) adding 1ml of water into a test tube, adding 1ml of bromine carbon tetrachloride solution, adding 1ml of test sample solution, fully oscillating, judging that the test sample passes olefinic bond identification if the reddish brown in the test tube fades, and judging that the test sample does not pass olefinic bond identification if the reddish brown in the test tube does not fade.

In this example, the preparation of the bromine in carbon tetrachloride solution: taking 1ml of bromine, placing the bromine into a glass bottle which is plugged by vaseline, adding 50ml of carbon tetrachloride, and forcibly shaking up to obtain a bromine carbon tetrachloride solution.

If the test sample passes aldehyde group identification and olefinic bond identification at the same time, judging the test sample to be the aldehyde oil methanol solution meeting the requirements; and if the test sample cannot pass the aldehyde group identification and the olefinic bond identification at the same time, judging that the test sample does not meet the requirements.

The above-described embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way. Those skilled in the art can make many changes and modifications to the disclosed embodiments, or modify equivalent embodiments to practice the disclosed embodiments, without departing from the scope of the disclosed embodiments. Therefore, equivalent variations made according to the idea of the present invention should be covered within the protection scope of the present invention without departing from the contents of the technical solution of the present invention.

Claims

1. A method for identifying an aldehyde oil methanol solution, which is characterized by comprising the following steps: performing aldehyde group identification and olefinic bond identification on the test sample, and judging the test sample to be the aldehyde oil methanol solution meeting the requirements if the test sample simultaneously passes the aldehyde group identification and the olefinic bond identification; if the test sample cannot pass the aldehyde group identification and the olefinic bond identification at the same time, judging that the test sample does not meet the requirements; the aldehyde group identification comprises the following steps: taking a test sample solution, adding a 2, 4-dinitrophenylhydrazine test solution into the test sample solution, wherein the volume ratio of the test sample to the 2, 4-dinitrophenylhydrazine test solution is 1; the preparation of the 2, 4-dinitrophenylhydrazine test solution comprises the following steps: weighing 1.5g of 2, 4-dinitrophenylhydrazine, adding 20ml of sulfuric acid solution (1 → 2), dissolving, adding water to 100ml, and filtering to obtain a 2, 4-dinitrophenylhydrazine test solution;

2. The method of claim 1, wherein the method comprises the steps of: during the identification of the olefinic bond, the volume ratio of water, bromine in carbon tetrachloride and the test sample is 1.

3. The method for identifying an aldehyde oil methanol solution according to any one of claims 1 or 2, characterized in that: preparation of the test sample: equal volume of aldehyde oil and methanol are taken and mixed evenly.

4. The method of claim 1, wherein the method comprises the steps of: preparing a bromine carbon tetrachloride solution: taking 1ml of bromine, placing the bromine into a glass bottle which is plugged by vaseline, adding 50ml of carbon tetrachloride, and forcibly shaking up to obtain a bromine carbon tetrachloride solution.